质谱学报2012，Vol.33Issue(4)：232-236,5.
同位素稀释-超高效液相色谱-串联质谱技术分析婴儿配方奶粉中的维生素D
Determination of Vitamin D in Infant Milk Powder by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry with Isotopes Dilution
摘要
Abstract
In order to establish a reliable method for quantitative analysis of vitamin D in infant milk powder, a ultra performance liquid chromatography-tandem mass spectrometry (UPLC/MS/MS) with isotopes dilution method was developed. The samples were sapon-ifed with KOH and extracted by pentane-ethyl ether solution (V(pentane):V(ethyl ether) = 4:1). The target analytes were separated on the Waters T3 column with gradient elution using methanol and water (containing 2 mmol/L ammonium formate for both) as mobile phase. The identification and quantification were achieved by using electrospray ionization in positive ion mode and with multiple reaction monitoring. Internal standard method was used to determine the results. The linear range of the calibration curve was 5-150 /μg/L. The limit of detection (LOD) of the method was 1. 5μg/kg, and the limit of quantitation (LOQ) was 5. 0μg/kg. The recoveries of the method were in the range of 97. 0% -104. 7% and 92. 7%-108. 0% for vitamin D2 and vitamin D3 respectively. The relative standard deviations (RSD) of intra-day and inter-day were less than 10%. The simply, rapid, accurate and sensitive method can be applied to determine the vitamin D in infant milk powder.关键词
同位素稀释/超高效液相色谱-串联质谱/维生素D/婴儿配方奶粉Key words
isotopes dilution/ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) /vitamin D/infant milk powder分类
化学化工引用本文复制引用
曹慧,陈小珍,王瑾,陈万勤..同位素稀释-超高效液相色谱-串联质谱技术分析婴儿配方奶粉中的维生素D[J].质谱学报,2012,33(4):232-236,5.基金项目
浙江省科技厅分析测试科技计划(2011C37072)、浙江省质量技术监督系统科研计划(20110203)项目资助 （2011C37072）
